Multiplug filtration clean‐up with multiwalled carbon nanotubes in the analysis of pesticide residues using LC–ESI‐MS/MS

Abstract

A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs < 15%. Matrix-matched calibrations were performed with the coefficients of determination >0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples.

Comparison of pulse glow discharge‐ion mobility spectrometry and liquid chromatography with tandem mass spectrometry based on multiplug filtration cleanup for the analysis of tricaine mesylate residues in fish and water

“…PSA is a weak anion exchanger that can remove various organic acids, fatty acids, and some sugars, and C 18 can absorb weak polarity substances like lipids . MWCNTs have been applied as effective clean‐up sorbents for removing fatty acids, pigments, and other matrix compounds in pesticide multiresidue analysis in our previous work . To obtain the best cleanup performance, different amounts of PSA, C 18 and MWCNTs were investigated in the m‐PFC procedure (combination A: 50 mg of PSA and 150 mg of MgSO 4 ; combination B: 100 mg of PSA and 150 mg of MgSO 4 ; combination C: 50 mg of PSA, 30 mg of C 18 , and 150 mg of MgSO 4 ; combination D: 30 mg of PSA, 30 mg of C 18 , 5 mg of MWCNTs, and 150 mg of MgSO 4 ).…”

“…PSA is a weak anion exchanger that can remove various organic acids, fatty acids, and some sugars, and C 18 can absorb weak polarity substances like lipids [21,22]. MWCNTs have been applied as effective clean-up sorbents for removing fatty acids, pigments, and other matrix compounds in pesticide multiresidue analysis in our previous work [18][19][20]. To obtain the best cleanup performance, different amounts of PSA, C 18 As shown in Fig.…”

Multiplug filtration cleanup method with multi-walled carbon nanotubes for the analysis of malachite green, diethylstilbestrol residues, and their metabolites in aquatic products by liquid chromatography–tandem mass spectrometry

“…The sorbent in the tip was 10 mg of MWCNTs mixed with 150 mg of MgSO 4 . The schematic diagrams of an m-PFC tip and the procedures were documented in our previous study [18]. The syringe needle was kept under the surface of extract, then the syringe piston was pulled and pushed for three times to let the extracts pass through the sorbents for the purpose of cleaning-up.…”

Dual‐layer column filtration cleanup and gas chromatography‐tandem mass spectrometry detection for the analysis of 39 pesticide residues in porcine meat

“…developed a high‐throughput method based on d‐SPE cleanup combined with in‐vial filtration for analysis of animal tissue . In our previous study, a rapid multiplug filtration cleanup (m‐PFC) method was employed for purification of nontarget compounds in various plant matrices . The m‐PFC method provided a more practical and effective way to perform the cleanup process than traditional d‐SPE method.…”